Copper sulfide anode and preparation method thereof

A copper sulfide and positive electrode technology, applied in battery electrodes, electrical components, circuits, etc., can solve the problems of unfavorable large-area preparation, long preparation cycle, and high equipment requirements, so as to improve cycle stability, avoid long-term reaction, and conduction performance Good results

Inactive Publication Date: 2013-07-24

XIANGTAN UNIV

3 Cites 19 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Therefore, an integrated porous electrode with a three-dimensional structure has a good prospect for lithium-sulfur batteries. However, at present, the preparation of integrated electrodes ...

Abstract

The invention provides a copper sulfide anode and a preparation method thereof, solving the problems of the conventional copper sulfide electrode that the bonding force of active substances and current collectors is poor and the anode conductivity is lowered because of a binder and also solving the problems of the integrated copper sulfide electrode which is synthesized in situ in a solution that the quantity of active substances is small and the preparation period is long. The copper sulfide anode is prepared by the following steps: uniformly spreading elemental sulfur which is prepared according to the sulfur carrying amount of foamy copper is 0.03-0.3g/cm<2> on the foamy copper, putting into a furnace, and carrying out in-situ reaction under a protection gas at a temperature of 155-350 DEG C so as to obtain the laminated copper sulphide which takes a foamy copper three-dimensional network structure as a framework, namely an integrated porous copper sulphide anode. By utilizing the copper sulfide anode, the application of the three-dimensional structured integrated porous anode in a lithium battery is widened, the energy density of a lithium battery anode is improved, and the performances of a lithium battery are improved. The copper sulfide anode is simple in preparation process, low in equipment requirement, low in cost and convenient for industrial production.

Application Domain

Cell electrodes

Technology Topic

In situ reactionCurrent collector +10

Image

Examples

Experimental program(3)
Comparison scheme(1)

Example Embodiment

[0048] Example 1

[0049] Preparation of copper sulfide integrated positive electrode: cut the foamed copper with a porosity of 94%, a pore diameter of 0.2mm, and a thickness of 2.5mm into discs with a diameter of 10mm, and press it to 0.2mm with a tablet press, and in 1mol/L HCl Use ultrasonic cleaning in the solution for 15 minutes, then ultrasonic cleaning in acetone solution for 15 minutes, and ultrasonic cleaning in deionized water for 10 minutes. The sulfur load is 0.03g/cm 2 Prepare foamed copper and elemental sulfur, weigh 2.9 mg of elemental sulfur ground to 50 μm, cover the elemental sulfur evenly on the foamed copper, place it in a tube furnace, and under the protection of nitrogen flow, the gas flow rate is 1.5 L/min, the flow rate 20cm/min; keep warm at 155°C for 3h, then raise the temperature to 350°C, keep warm for 1h, synthesize lamellar copper sulfide on the foamed copper skeleton, and the copper sulfide on the sheet has a snowflake-like shape, that is, the positive electrode, the copper sulfide in the positive electrode The thickness of the lamellae is about 200-300 nm, and the interlamellar distance is about 1.5-2 μm.

[0050] The assembly and test of lithium-sulfur battery: the copper sulfide positive electrode that obtains with embodiment 1 is used as positive electrode, lithium metal is used as negative electrode, and shell cover adopts CR2032 type, and electrolytic solution adopts LiTFSI/DOL:DEM (1:1 volume ratio of 1mol/L, DOL: 1,3-dioxolane; DME: ethylene glycol dimethyl ether), the separator is Celgard2400; a button lithium-sulfur battery is assembled in an argon atmosphere glove box. Use the Xinwei battery test system to test the battery performance, the test temperature is room temperature, and the charge and discharge voltage is relative to Li/Li + The charge and discharge rate of the test is 0.2C, and the cycle is 100 times. The charge and discharge specific capacity of the copper sulfide positive electrode described in the present invention is calculated by the mass of the integrated electrode.

Example Embodiment

[0051] Example 2

[0052] Preparation of copper sulfide integrated positive electrode: Cut the foamed copper with a porosity of 96%, a pore diameter of 0.15 mm, and a thickness of 2.7 mm into discs with a diameter of 10 mm, and press it to 0.3 mm with a tablet press. Use ultrasonic cleaning in HCl solution for 30 minutes, then ultrasonic cleaning in acetone solution for 30 minutes, and ultrasonic cleaning in deionized water for 15 minutes. According to the sulfur loading capacity of foamed copper is 0.18g/cm 2 Prepare foamed copper and elemental sulfur, weigh 17.5 mg of elemental sulfur ground to 10 μm, cover the elemental sulfur evenly on the foamed copper, place it in a tube furnace, and under the protection of argon gas flow, the gas flow rate is 0.1L/min. The flow rate is 2cm/min; heat preservation at 155°C for 8 hours, and the lamellar copper sulfide is synthesized on the foamed copper skeleton. The copper sulfide on the sheet has a hexagonal columnar shape, and the positive electrode is obtained. 200nm, the lamellar spacing is about 1-1.5μm.

[0053] The lithium-sulfur battery was assembled and tested in the same manner as in Example 1. Use the Xinwei battery test system to test the battery performance, the test temperature is room temperature, and the charge and discharge voltage is relative to Li/Li + The charge and discharge rate of the test is 0.2C, and the cycle is 100 times. The charge and discharge specific capacity of the copper sulfide positive electrode described in the present invention is calculated by the mass of the integrated electrode. Using the Shanghai Chenhua Electrochemical Workstation, the cyclic voltammetry test was carried out on the battery after 100 cycles, the test voltage was 1-3V, and the scan rate was 10mA.

Example Embodiment

[0054] Example 3

[0055] Preparation of copper sulfide integrated positive electrode: foamed copper with a porosity of 98%, a pore diameter of 0.1mm, and a thickness of 3mm is cut into a disc with a diameter of 10mm, pressed to 0.5mm with a tablet press, and placed in a 2mol/L HCl solution Use ultrasonic cleaning for 60 minutes, then ultrasonic cleaning in acetone solution for 60 minutes, ultrasonic cleaning in deionized water for 20 minutes, the power of ultrasonic wave is 100W, vacuum dry the cleaned foamed copper at 80°C for 40 minutes, and set aside; The amount is 0.3g/cm 2 Prepare foamed copper and elemental sulfur, weigh 29 mg of elemental sulfur ground to 100 μm, cover the elemental sulfur evenly on the foamed copper, place it in a tube furnace, and under the protection of an argon atmosphere, the gas flow rate is 5 L/min, and the flow rate is 60cm/min; heat preservation at 155°C for 2 hours, heat preservation at 250°C for 1 hour, synthesize sheet-like copper sulfide on the foamed copper skeleton, and the copper sulfide on the sheet has a snowflake-like shape, and the positive electrode is obtained. The thickness of the copper sulfide sheet in the positive electrode is about It is 100-200nm, and the lamellar spacing is about 1.5-2μm.

[0056] The lithium-sulfur battery was assembled in the same manner as in Example 1. Use the Xinwei battery test system to test the charge and discharge performance and rate stability of the assembled battery. The test temperature is room temperature, and the charge and discharge voltage is relative to Li/Li + It is 1~3V, and the charge and discharge rate is 0.2C, 0.5C, 1C, 0.5C, 0.2C, 0.5C in sequence.

PUM

Property	Measurement	Unit
Sheet thickness	100.0 ~ 300.0	nm
Average pore size	100.0 ~ 200.0	µm
Thickness	2.5 ~ 3.0	mm

Description & Claims & Application Information

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Copper sulfide anode and preparation method thereof

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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